	US 11,733,199 B2
	Fabrication method of enzyme-free glucose sensor and use of enzyme-free glucose sensor fabricated by the same
Quan Bu, Jiangsu (CN); Jin Cai, Jiangsu (CN); Hairong Long, Jiangsu (CN); Mei Wang, Jiangsu (CN); and Hanping Mao, Jiangsu (CN)
Assigned to Jiangsu University, Jiangsu (CN)
Appl. No. 17/610,443
Filed by Jiangsu University, Jiangsu (CN)
PCT Filed Apr. 30, 2021, PCT No. PCT/CN2021/091372 § 371(c)(1), (2) Date Nov. 11, 2021, PCT Pub. No. WO2022/062409, PCT Pub. Date Mar. 31, 2022.
Claims priority of application No. 202011013417.3 (CN), filed on Sep. 24, 2020.
Prior Publication US 2022/0341868 A1, Oct. 27, 2022
Int. Cl. G01N 27/327 (2006.01); G01N 27/30 (2006.01); G01N 27/416 (2006.01)

CPC G01N 27/3277 (2013.01) [G01N 27/308 (2013.01); G01N 27/3278 (2013.01); G01N 27/4163 (2013.01)]

8 Claims

1. A fabrication method of an enzyme-free glucose sensor, comprising the following specific steps:

step (1): subjecting washed and dried Magnolia grandiflora L. leaves to calcination in a high-temperature tube furnace to obtain a biochar;

step (2): soaking the biochar in hydrochloric acid, adding the hydrochloric acid-treated biochar, pyromellitic acid, nickel acetylacetonate, and N,N-dimethylformamide to a mixed solution of ethanol and ultrapure water to obtain a resulting mixture, and stirring the resulting mixture for dispersion to obtain a mixed solution A;

step (3): subjecting the mixed solution A to a reaction in a microwave synthesizer to obtain a mixed solution precursor B, wherein in the step (3), the reaction in the microwave synthesizer is conducted under the following process parameters: a microwave power: 180 W to 200 W, a reaction temperature: 160° C. to 180° C., and a reaction time: 2 h;

step (4): pouring the mixed solution precursor B into a centrifuge tube, then centrifuging and drying the mixed solution precursor B to obtain a product C;

step (5): flowing NH₃in the high-temperature tube furnace and subjecting the product C to high-temperature calcination at 900° C. for 2 h in the high-temperature tube furnace to obtain a Ni@NSiC nano-electrode composite material; and

step (6): mixing the Ni@NSiC nano-electrode composite material, water, ethanol, and a 5 wt % Nafion solution to prepare a Ni@NSiC solution, pipetting the Ni@NSiC solution with a pipette and adding dropwise onto a pretreated electrode, and air-drying the electrode to obtain a Ni@NSiC/GCE electrode,

wherein in the step (6), in the Ni@NSiC solution, the Ni@NsiC nano-electrode composite material has a concentration of 5 mg/mL, and the water, the ethanol, and the 5 wt % Nafion solution have a volume ratio of 665 μL:335 μL:25 μL; 5 μL of the Ni@NsiC solution is pipetted with the pipette; and the pretreated electrode is prepared by polishing a glassy carbon electrode (GCE) successively with 1.0 μm, 0.3 μm, and 0.05 μm Al₂O₃polishing powders; rinsing the GCE with deionized water, and subjecting the GCE to ultrasonic treatment three times with deionized water and then to ultrasonic treatment once with absolute ethanol, wherein each ultrasonic treatment is conducted for no more than 30 s; and finally blow-drying the GCE with nitrogen.